Propargyl bromide → 4-Methyl-1-(prop-2-yn-1-yl)piperidine

HRID 6791

반응식

HRID 6791 반응식
[CH2:1](Br)[C:2]#[CH:3].[CH3:5][CH:6]1[CH2:11][CH2:10][NH:9][CH2:8][CH2:7]1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH3:5][CH:6]1[CH2:11][CH2:10][N:9]([CH2:3][C:2]#[CH:1])[CH2:8][CH2:7]1

참가 물질

5

반응물 3

HCID 7842Propargyl bromideHCID 11430Potassium CarbonateHCID 693814-Methylpiperidine

생성물 1

HCID 113555094-Methyl-1-(prop-2-yn-1-yl)piperidine수율 92%

시약·촉매·용매 1

HCID 180Acetone용매

반응 조건

온도
50 °C

실험 절차

At 0–5° C., propargyl bromide (12.01 g) was added dropwise with stirring to a suspension of 4-methylpiperidine (10.0 g) and potassium carbonate (13.96 g) in dry acetone (80 ml). The mixture was stirred at 50° C. for 6 hours and then filtered. The filtrate was concentrated under reduced pressure and the residue was taken up in dichloromethane. The organic phase was washed with water (3×15 ml), dried with sodium sulfate and concentrated under reduced pressure. Distillation of the residue under reduced pressure gave 12.73 g of an oil of boiling point 60° C./16 mm Hg.

후처리

  1. filtrationfiltered
  2. concentrationThe filtrate was concentrated under reduced pressure
  3. washThe organic phase was washed with water (3×15 ml)
  4. dry with materialdried with sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. distillationDistillation of the residue under reduced pressure

출처 및 근거

ORD 기록
ord-3d1eef909b754b8da0b694cdccfec3a6
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07084158B2

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